CN106044808A - Production method for recovering magnesium sulfate from boric acid mother liquor - Google Patents
Production method for recovering magnesium sulfate from boric acid mother liquor Download PDFInfo
- Publication number
- CN106044808A CN106044808A CN201610650520.6A CN201610650520A CN106044808A CN 106044808 A CN106044808 A CN 106044808A CN 201610650520 A CN201610650520 A CN 201610650520A CN 106044808 A CN106044808 A CN 106044808A
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- China
- Prior art keywords
- boric acid
- magnesium sulfate
- liquid
- mother liquor
- boron
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1045—Oxyacids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a production method for recovering magnesium sulfate from a boric acid mother liquor. The method mainly comprises the processes of mother liquor purification, concentration, crystallization and floatation. The method improves the boric acid yield in the boric acid production process to 85% or above from present 77%, effectively recovers the magnesium sulfate product, and allows 147t of boric acid and 980t of magnesium sulfate to be recovered if 1000t of boron is produced every year (the magnesium sulfate is mainly recovered from Tibetan szaibelyite, and boric acid is only recovered from other low-magnesium boron rocks. The method has the advantages of simple process, small investment, solving of the problem of mother liquor recovery, boron resource saving, environment pollution reduction, and good social and economic benefits.
Description
The present invention relates to a kind of production method reclaiming magnesium sulfate from mother liquid of boric acid.
Sulfuric acid process is that the boron rock (kurnakovite ore deposit, hydroboracite ore deposit, pinnoite ore deposit) of using being widely used at present produces
The method of boric acid, its feature is that resolution ratio is high (98.5-99.6%), but subject matter is the yield low (70-77%) of boric acid,
Mother solution amount is big, and mother solution mesoboric acid separates more difficult with magnesium sulfate, produces 1 ton of boric acid, and about discharge 4-6 ton mother solution, about damages
Lose 0.15 ton of boric acid, 1 ton of magnesium sulfate, for the utilization of mother solution, be so far to, domestic and international experts and scholars have made many research, remove
Some areas and manufacturer are processed into outside boric magnesium fertilizer, and remaining Technology reclaiming and comprehensively utilizing is showed no and realizes work
The report of industry.Mother solution problem always perplexs a great problem of domestic and international boric acid manufacturing enterprise, and boron is a kind of non-renewable
Resource, the discharge of a large amount of mother solutions, had both caused the waste of boron resource, and had polluted again environment.
It is an object of the invention to solve the problem that during boric acid produces, disposing mother liquor utilizes, improve the yield of boric acid, and return
Receive magnesium sulfate, reduce environmental pollution, save boron resource.
The technical scheme that the present invention intends taking is: a kind of production method reclaiming magnesium sulfate from mother liquid of boric acid, its feature
Being that it is made up of following process, mother liquid of boric acid concentrates after refined, is concentrated to feed liquid Baume degrees when being 25-50, enters cooling
Crystallization, crystallization time is 5-36 hour, then adds flotation agent and carry out flotation, and the thick boric acid floatingly selected enters the acidolysis during boric acid produces
Carrying out boric acid production in groove, in flotation device, remaining material enters solid-liquid separation in entering centrifugal separator, and solid is magnesium sulfate
Product, liquid returns and mixes continuation concentration in enrichment process with mother liquid of boric acid.Present invention is generally directed to Tibet boron rock and reclaim sulphuric acid
Magnesium, other low magnesium boron rock only reclaims boric acid.
The present invention has the loss making boric acid produce mother solution mesoboric acid and greatly reduces, and obtains qualified Magnesium sulfate heptahydrate industry
Product.Make the technique discharge simply boron mud discharge of whole Production By Sulfuric Acid Process boric acid, not only make the magnesium sulfate in mother solution be recycled, with
Time, make the yield of boric acid bring up to more than 85%, decrease the waste of boron resource, solve problem of environmental pollution, for sulfuric acid process
Liao Yitiaoxin road is explored in the disposing mother liquor utilization producing boric acid generation, based on boric acid production scale 1000 tons/year, and recyclable boron
Acid 147 tons, 980 tons of magnesium sulfate.It is strong that the present invention has the suitability, and technique is simple, easy and simple to handle, invests little, economic results in society
The advantage such as good.
The invention will be further described below in conjunction with the accompanying drawings.
Accompanying drawing is present invention process flow diagram.
First filter boric acid production process obtains ground mother solution filter cloth, remove the impurity such as silt, ferrum, complete mother
Liquid subtractive process, mother solution composition now is about 3% boric acid, 20% magnesium sulfate, above-mentioned mother solution is squeezed into evaporation equipment and steams
Send out and concentrate, be concentrated to feed liquid Baume degrees when being 25-50, stop concentrating.Feed liquid is squeezed in crystallizer, crystallisation by cooling 5-36 hour
After, then slip to be squeezed into flotation device carries out flotation, during flotation, add flotation agent, flotation agent is conventional secondary amine, terpineol, shallow lake
The complexing agent of powder, thick boric acid is flotated under the effect of flotation device by slip, and thick boric acid returns in the acidolysis groove that boric acid produces
Entering boric acid production process, the feed liquid in flotation device enters and carries out solid-liquid separation from extension set, and the centrifugal magnesium salt obtained is scrubbed, dries in the air
The dry magnesium sulfate product obtaining meeting HG/T2688-95 standard, filtrate again returns to the enrichment process recycling of the present invention.
It is below several embodiments of the present invention.
Embodiment 1:
Weigh 3.5 kilograms of mother liquid of boric acid, analyze and measure (H3BO3%=3.24MgSO4%=18.55), through vacuum filtration,
Removing impurity and ferrum etc., evaporation and concentration on electric furnace, stop evaporation and concentration when feed liquid Baume degrees is 27, crystallisation by cooling is after 6 hours,
Weigh the material 1.5 kilograms of advantages of good crystallization, put into and flotation cell carries out flotation, be simultaneously introduced flotation agent, i.e. 3 grams secondary amine, 1.5 grams of pines
Oleyl alcohol, 4.5 grams of starch, after roughly selecting for ten a few minutes, be continuously added mother liquid of boric acid 400 grams and scan, and after about ten minutes, stops floating
Choosing, the feed liquid floatingly selected is centrifuge dripping after foam merges, and filter cake weighs 145 grams, analyzes and measures, wherein H3BO3%=15.37,
MgSO4%=38.50, feed liquid centrifuge dripping again in flotation cell, filter cake weighs 405 grams, analyzes and measures, H3BO3%=0.7,
MgSO4%=97.79, two parts filtrate combined analysis measures H3BO3%=2.42.
Embodiment 2:
Taking 4.6 cubic metres of mother liquid of boric acid, machine filters by centrifugation, removes the impurity such as ferrum, puts into and concentrate in evaporation boiler, material
When liquid Baume degrees is 40, stop concentrating, with pump, concentrated solution is squeezed into cooling in crystallizer, after about 20 hours, feed liquid is squeezed into floating
Select and machine carries out flotation, be simultaneously introduced flotation agent, be i.e. secondary amine 4.6 kilograms, terpineol 2.3 kilograms, starch 4.5 kilograms, roughly select 10
After minute, being continuously added mother solution and scan, the material flotated returns and enters boron in the acidolysis groove in boric acid production process
Acid produces, and material in flotation device enters in centrifuge and carries out solid-liquid separation, and filtrate returns to continue in the enrichment process of the present invention
Concentrating, filter cake is magnesium sulfate (MgSO4·7H2O) product, it is heavy is 170 kilograms, measures filter cake analysis, wherein H3BO3%
=O.55, MgSO4·7H2O%=97.66, product meets magnesium sulfate national standard.
Embodiment 3:
Taking 10 cubic metres of mother liquid of boric acid, mother solution centrifugation refines, and removes impurity, is concentrated to feed liquid Baume in concentration pan
Degree 48, squeezes into crystallizer, crystallisation by cooling 34 hours, and other operation, with embodiment 2, obtains magnesium sulfate (MgSO4·7H2O) product
400Mg, measures through analyzing, wherein H3BO3%=0.36, MgSO4·7H2O%=98.82, product meets magnesium sulfate country mark
Accurate.
Claims (1)
1. the production method reclaiming magnesium sulfate from mother liquid of boric acid, it is characterised in that it is made up of following process, boric acid is female
Liquid concentrates after refined, is concentrated to feed liquid Baume degrees when being 25-50, enters crystallisation by cooling, and crystallization time is 5-36 hour, then adds
Flotation agent carries out flotation, and the thick boric acid floatingly selected enters in the acidolysis groove during boric acid produces and carries out boric acid production, surplus in flotation device
Under material enter in centrifugal separator and carry out solid-liquid separation, solid is magnesium sulfate product, liquid return in enrichment process with
Mother liquid of boric acid mixing continues to concentrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610650520.6A CN106044808A (en) | 2016-08-09 | 2016-08-09 | Production method for recovering magnesium sulfate from boric acid mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610650520.6A CN106044808A (en) | 2016-08-09 | 2016-08-09 | Production method for recovering magnesium sulfate from boric acid mother liquor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106044808A true CN106044808A (en) | 2016-10-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610650520.6A Pending CN106044808A (en) | 2016-08-09 | 2016-08-09 | Production method for recovering magnesium sulfate from boric acid mother liquor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107638960A (en) * | 2017-08-25 | 2018-01-30 | 中国科学院青海盐湖研究所 | The method of separating boron |
| CN108203099A (en) * | 2016-12-19 | 2018-06-26 | 临沂大学 | The combination device of residual heat resources comprehensive reutilization during a kind of low-grade boron magnesium ore production boric acid |
| CN110357119A (en) * | 2019-08-26 | 2019-10-22 | 东北大学 | A kind of new method using magnesium sulfate in non-evaporative crystallization method removing boric acid solution |
| CN110510626A (en) * | 2019-08-06 | 2019-11-29 | 东北大学 | It is a kind of to utilize SO2The method of gas-selectively leaching boron magnesium ore |
-
2016
- 2016-08-09 CN CN201610650520.6A patent/CN106044808A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108203099A (en) * | 2016-12-19 | 2018-06-26 | 临沂大学 | The combination device of residual heat resources comprehensive reutilization during a kind of low-grade boron magnesium ore production boric acid |
| CN108203099B (en) * | 2016-12-19 | 2023-02-21 | 临沂大学 | Combined equipment for comprehensively recycling waste heat resources in process of producing boric acid from low-grade boron magnesium ore |
| CN107638960A (en) * | 2017-08-25 | 2018-01-30 | 中国科学院青海盐湖研究所 | The method of separating boron |
| CN107638960B (en) * | 2017-08-25 | 2019-11-22 | 中国科学院青海盐湖研究所 | The method of separating boron |
| CN110510626A (en) * | 2019-08-06 | 2019-11-29 | 东北大学 | It is a kind of to utilize SO2The method of gas-selectively leaching boron magnesium ore |
| CN110357119A (en) * | 2019-08-26 | 2019-10-22 | 东北大学 | A kind of new method using magnesium sulfate in non-evaporative crystallization method removing boric acid solution |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161026 |
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| WD01 | Invention patent application deemed withdrawn after publication |